Laboratory Medicine ›› 2020, Vol. 35 ›› Issue (8): 811-817.DOI: 10.3969/j.issn.1673-8640.2020.08.016
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ZOU Jihua1, LI Quanle1, SHEN Min1, ZHANG Man2, YANG Xiaodong1, TU Minmin1, FENG Dongfang3, SUN Hongna1
Received:
2020-02-13
Online:
2020-08-30
Published:
2020-09-24
CLC Number:
ZOU Jihua, LI Quanle, SHEN Min, ZHANG Man, YANG Xiaodong, TU Minmin, FENG Dongfang, SUN Hongna. Establishment and performance evaluation of candidate reference measurement procedure for serum aldosterone by liquid chromatography-tandem mass spectrometry[J]. Laboratory Medicine, 2020, 35(8): 811-817.
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名称 | 测定方式 | 母离子/(m/z) | 子离子/(m/z) | 驻留时间/ms | 去簇电压/V | 碰撞电压/V |
---|---|---|---|---|---|---|
醛固酮 | 定量 | 359.2 | 189.1 | 270 | -110 | -25 |
定性 | 359.2 | 331.2 | 270 | -110 | -22 | |
醛固酮-2H7 | 定量 | 366.2 | 194.1 | 270 | -110 | -25 |
定性 | 366.2 | 338.2 | 270 | -110 | -21 |
名称 | 测定方式 | 母离子/(m/z) | 子离子/(m/z) | 驻留时间/ms | 去簇电压/V | 碰撞电压/V |
---|---|---|---|---|---|---|
醛固酮 | 定量 | 359.2 | 189.1 | 270 | -110 | -25 |
定性 | 359.2 | 331.2 | 270 | -110 | -22 | |
醛固酮-2H7 | 定量 | 366.2 | 194.1 | 270 | -110 | -25 |
定性 | 366.2 | 338.2 | 270 | -110 | -21 |
样本类型 | 样本数 | 醛固酮/(nmol/L) | CI/QI比值平均值 (范围) |
---|---|---|---|
标准溶液 | 63 | 0.08~3.55 | 0.71(0.62~0.77) |
血清 | 90 | 0.11~3.15 | 0.69(0.61~0.78) |
样本类型 | 样本数 | 醛固酮/(nmol/L) | CI/QI比值平均值 (范围) |
---|---|---|---|
标准溶液 | 63 | 0.08~3.55 | 0.71(0.62~0.77) |
血清 | 90 | 0.11~3.15 | 0.69(0.61~0.78) |
样本编号 | 理论值/(nmol/L) | 样本数 | 测定均值/(nmol/L) | 平均RSN | CV/% | 偏移/% |
---|---|---|---|---|---|---|
1 | 0.075 | 10 | 0.083 | 39 | 6.32 | 5.60 |
2 | 0.056 | 10 | 0.064 | 27 | 8.69 | 10.28 |
3 | 0.045 | 10 | 0.052 | 15 | 13.88 | 12.56 |
样本编号 | 理论值/(nmol/L) | 样本数 | 测定均值/(nmol/L) | 平均RSN | CV/% | 偏移/% |
---|---|---|---|---|---|---|
1 | 0.075 | 10 | 0.083 | 39 | 6.32 | 5.60 |
2 | 0.056 | 10 | 0.064 | 27 | 8.69 | 10.28 |
3 | 0.045 | 10 | 0.052 | 15 | 13.88 | 12.56 |
样本 | 批次 | 平均值/(nmol/L) | 批内CV/% | 批间CV/% | 总体平均值/(nmol/L) |
---|---|---|---|---|---|
低浓度 | 1 | 0.211 | 4.70 | 4.09 | 0.213 |
2 | 0.206 | 4.97 | |||
3 | 0.223 | 3.14 | |||
中浓度 | 1 | 1.298 | 2.47 | 2.76 | 1.284 |
2 | 1.243 | 2.50 | |||
3 | 1.310 | 3.18 | |||
高浓度 | 1 | 2.832 | 0.78 | 2.28 | 2.839 |
2 | 2.779 | 1.09 | |||
3 | 2.907 | 0.96 |
样本 | 批次 | 平均值/(nmol/L) | 批内CV/% | 批间CV/% | 总体平均值/(nmol/L) |
---|---|---|---|---|---|
低浓度 | 1 | 0.211 | 4.70 | 4.09 | 0.213 |
2 | 0.206 | 4.97 | |||
3 | 0.223 | 3.14 | |||
中浓度 | 1 | 1.298 | 2.47 | 2.76 | 1.284 |
2 | 1.243 | 2.50 | |||
3 | 1.310 | 3.18 | |||
高浓度 | 1 | 2.832 | 0.78 | 2.28 | 2.839 |
2 | 2.779 | 1.09 | |||
3 | 2.907 | 0.96 |
样本 | 加标浓度/(nmol/L) | 血清平均浓度/(nmol/L) | 测得浓度/(nmol/L) | 回收率/% | 平均回收率/% | CV/% |
---|---|---|---|---|---|---|
低浓度 | ||||||
L-1 | 0.203 | 0.362 | 0.563 | 99.01 | 98.52 | 1.87 |
L-2 | 0.561 | 98.03 | ||||
L-3 | 0.565 | 100.00 | ||||
L-4 | 0.563 | 99.01 | ||||
L-5 | 0.555 | 95.07 | ||||
L-6 | 0.565 | 100.00 | ||||
中浓度 | ||||||
M-1 | 1.084 | 0.362 | 1.430 | 98.52 | 99.09 | 1.21 |
M-2 | 1.458 | 101.11 | ||||
M-3 | 1.422 | 97.79 | ||||
M-4 | 1.435 | 98.99 | ||||
M-5 | 1.444 | 99.82 | ||||
M-6 | 1.428 | 98.34 | ||||
高浓度 | ||||||
H-1 | 2.701 | 0.362 | 3.031 | 98.82 | 100.14 | 1.67 |
H-2 | 3.048 | 99.44 | ||||
H-3 | 3.005 | 97.85 | ||||
H-4 | 3.101 | 101.41 | ||||
H-5 | 3.100 | 101.37 | ||||
H-6 | 3.116 | 101.96 |
样本 | 加标浓度/(nmol/L) | 血清平均浓度/(nmol/L) | 测得浓度/(nmol/L) | 回收率/% | 平均回收率/% | CV/% |
---|---|---|---|---|---|---|
低浓度 | ||||||
L-1 | 0.203 | 0.362 | 0.563 | 99.01 | 98.52 | 1.87 |
L-2 | 0.561 | 98.03 | ||||
L-3 | 0.565 | 100.00 | ||||
L-4 | 0.563 | 99.01 | ||||
L-5 | 0.555 | 95.07 | ||||
L-6 | 0.565 | 100.00 | ||||
中浓度 | ||||||
M-1 | 1.084 | 0.362 | 1.430 | 98.52 | 99.09 | 1.21 |
M-2 | 1.458 | 101.11 | ||||
M-3 | 1.422 | 97.79 | ||||
M-4 | 1.435 | 98.99 | ||||
M-5 | 1.444 | 99.82 | ||||
M-6 | 1.428 | 98.34 | ||||
高浓度 | ||||||
H-1 | 2.701 | 0.362 | 3.031 | 98.82 | 100.14 | 1.67 |
H-2 | 3.048 | 99.44 | ||||
H-3 | 3.005 | 97.85 | ||||
H-4 | 3.101 | 101.41 | ||||
H-5 | 3.100 | 101.37 | ||||
H-6 | 3.116 | 101.96 |
样本 | 实验室编号/(nmol/L) | 均值/ (nmol/L) | 偏移/% | ||||
---|---|---|---|---|---|---|---|
1 | 2 | 3 | 4 | 5 | |||
RELA-A | 1.697 | 1.703 | 1.688 | 1.730 | 1.641 | 1.692 | -0.22 |
RELA-B | 1.305 | 1.322 | 1.286 | 1.360 | 1.257 | 1.306 | -1.53 |
样本 | 实验室编号/(nmol/L) | 均值/ (nmol/L) | 偏移/% | ||||
---|---|---|---|---|---|---|---|
1 | 2 | 3 | 4 | 5 | |||
RELA-A | 1.697 | 1.703 | 1.688 | 1.730 | 1.641 | 1.692 | -0.22 |
RELA-B | 1.305 | 1.322 | 1.286 | 1.360 | 1.257 | 1.306 | -1.53 |
样本组 | 峰面积比值 | 峰面积比值均值 | 相对基质效应/% | ||||
---|---|---|---|---|---|---|---|
第1次检测 | 第2次检测 | 第3次检测 | 第4次检测 | 第5次检测 | |||
A | 1.37 | 1.44 | 1.40 | 1.46 | 1.38 | 1.41 | |
B | 3.34 | 3.51 | 3.48 | 3.33 | 3.39 | 3.41 | |
C | 2.52 | 2.44 | 2.51 | 2.46 | 2.48 | 2.48 | 3.01 |
D | 3.05 | 3.11 | 3.16 | 3.10 | 3.16 | 3.12 | 3.52 |
E | 1.91 | 1.83 | 1.83 | 1.85 | 1.87 | 1.86 | 2.65 |
样本组 | 峰面积比值 | 峰面积比值均值 | 相对基质效应/% | ||||
---|---|---|---|---|---|---|---|
第1次检测 | 第2次检测 | 第3次检测 | 第4次检测 | 第5次检测 | |||
A | 1.37 | 1.44 | 1.40 | 1.46 | 1.38 | 1.41 | |
B | 3.34 | 3.51 | 3.48 | 3.33 | 3.39 | 3.41 | |
C | 2.52 | 2.44 | 2.51 | 2.46 | 2.48 | 2.48 | 3.01 |
D | 3.05 | 3.11 | 3.16 | 3.10 | 3.16 | 3.12 | 3.52 |
E | 1.91 | 1.83 | 1.83 | 1.85 | 1.87 | 1.86 | 2.65 |
样本编号 | 测定结果/(nmol/L) | 扩展不确定度/(nmol/L) | 相对扩展不确定度/% |
---|---|---|---|
1 | 0.225 | 0.01 | 4.44 |
2 | 1.286 | 0.07 | 5.36 |
3 | 1.688 | 0.08 | 4.62 |
样本编号 | 测定结果/(nmol/L) | 扩展不确定度/(nmol/L) | 相对扩展不确定度/% |
---|---|---|---|
1 | 0.225 | 0.01 | 4.44 |
2 | 1.286 | 0.07 | 5.36 |
3 | 1.688 | 0.08 | 4.62 |
项目 | 量值 | 标准不确定度 | 相对标准不确定度 |
---|---|---|---|
A/A内标 | 5.587 | 0.113 | 0.02 |
fc | 1.000 | 0.005 | 0.005 |
fm | 0.302 | 0.002 | 0.007 |
k | 2.740 | 0.018 | 0.006 |
b | 0.092 | 0 | 0 |
重复性/(ng/mL) | 0.608 | 0.001 | 0.002 |
测定均值/(nmol/L) | 1.688 | ||
合成相对标准不确定度/% | 2.310 | ||
扩展因子(95%可信区间) | 2.000 | ||
相对扩展不确定度/% | 4.620 |
项目 | 量值 | 标准不确定度 | 相对标准不确定度 |
---|---|---|---|
A/A内标 | 5.587 | 0.113 | 0.02 |
fc | 1.000 | 0.005 | 0.005 |
fm | 0.302 | 0.002 | 0.007 |
k | 2.740 | 0.018 | 0.006 |
b | 0.092 | 0 | 0 |
重复性/(ng/mL) | 0.608 | 0.001 | 0.002 |
测定均值/(nmol/L) | 1.688 | ||
合成相对标准不确定度/% | 2.310 | ||
扩展因子(95%可信区间) | 2.000 | ||
相对扩展不确定度/% | 4.620 |
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